The invention provides a preparation method of a 2,5-dialkoxyl dihydrofuran compound. The preparation method comprises the following steps: adding a furan compound shown by a formula I, alkyl alcohol shown by a formula III and an acid-binding agent into a reactor, stirring to react with chlorine, keeping the reaction temperature to be (-25)-25 DEG C, and reacting to obtain a 2,5-dialkoxyl dihydrofuran compound shown by a formula II, wherein in the formulas, R1, R2, R3 and R4 are independent hydrogen, halogen and C1-C5 alkyl, and R1 is a C1-C12 alkyl. The method provided by the invention is less in investment, low in energy consumption and high in efficiency; the reaction method is simple, and the operation is convenient and easy to implement; the raw materials are low in price, easy to obtain, and low in production cost; a byproduct is salt and can meet requirements on environmental protection; and the preparation method is suitable for performing industrial large-scale production of the 2,5-dialkoxyl dihydrofuran compound. Particularly, when a phase transfer catalyst is added into the method provided by the invention, the method also has the advantage that the yield of a target product is obviously improved.